Chemical reaction tower



Oct. 13, .1953 L. A. LEDGETT CHEMICAL REACTION TOWER Original Filed June 9, 1948 LOWELL A-LEDGETT Patented Oct. 13, 1953 e, 55,435 CHEMICAL REACTION TOWER. Lowell A. Ledgett, itidgewood, N. J assignor to Colgateel'al'molive-Peet Company,

N. J a corporationof Delaware Original application June 9, 1948, Serial No. 31,861. Divided and this application August 25,194f9, Serial Ne. 112,338

2 Claims. (01. ga -28,3)

This invention elates t qn m q reactions in which gas or heat or both gas and heat are liberated. preferred embodiment relates to a method of as ara us $91" WW facturing ce-ac i e a ents such a We tin emulsifying, dispersing, penetrating and deterging agents which contain salts of organic sulphonic acids. The invention relates more pare ticularly to improvements in the neutralization of the acid mix which facilitate maintaining the temperature of the reacting materials pract c n n despit the la amoun Q heat liberated in the reaction, and which alse iaciii ta removal f g s w th ut ex ssi e f m n i & gas'producing ne ralizi g a ent i u d- The neutralization of organic sulphgniciacids suitable for use as surface-active agents is an exothermic reaction which liberates a very sub; stantial amount Qfheat if this heat islnot cf,- fectively dissipated, the temperature cf the reacting mixture may rise suiiicientiy to cause excessive deterioration of the produet, particularly if pH is not maintained closely throughout the reaction mixture by rapid complete mixing of the reactants. Serious operating difiiculties may also be encountered in this and other exothermic reactions if tempera t lfi rise is not controlled. In a closed system, for example, dangerous pressures may be built up which are capable of destroying the apparatus. On the other handjif the a p r i o Pressu eale vol ti qomponents 0f h eac on mi ture ma 9W a before h r ction i tem les du o th large amount of heat liberated, thus causing foaming and lack of homogeneity in the mass, which may causeadditional local overheating. If carbonates or bicarbonates are used asneutralicing agents, the gases evolved as reaction products cause difiiculties such as interference with the operation of pumps,,foaming similar tothat experienced where volatile productsiiash ofl before completion of the reactiometc,

I h h r to ore bee maposcd t nt ol temperatures in neutralization reactigns bycause ing the reaction to take place in a circulating mass of the rea tiOI! m'oducts from which heat is removed through indirect heat exchangers, or by immediately vaporizing one or more volatile constituents from the reactionrproducts. Where indirect cooling is used, large heat transfer surfaces are required'to be fabricated frommaterials which are capable of withstanding corrosion by the substances employed in the reaction. When handlinganomalcus fluids with high fapparent visc0$il f fitt 1 attests-s lids in se stien is abstracted directly from the mass, the

asns tn et nd whe ntm mpe ature close to that at which crystallization, solidmama peris lti e c, o curs s Cow n is mer ea i l and ttq iomit tha l ate at xcha Wh e imm d e f ash cooling is e f ployedfliowever, it is not possible to provide prot n tame fia hi s befo omplet n 9 h r than an Suc yst m d e not ermi of sta e ntro the t t i a -sal e t i he ea ti n ma s stem m in exte al m he an u p n mqrt v a n t si Q t h ff h' rtt qlt rates throug a flas 0 especially 'under inherent conditions of high PQ l :21 in Plai s nt/9 ebra t in irateslhest and othe .q saq antases 9 i r P ae 1t a d p a tice .oyt' t mt by th re t aveati i whic reases an im ed rote t d ap ar n e the eutra iz n t in he l mitattu s r t tt t sweet-at agents, a wi b emelaapar i rom t t w h tai d s s ri' iqit an t t ac pan a e n hiti i' E lit a e ti na eleva i n of an a p r u embo yin th at nt n e a n t f t en utr i ati n ,r a t on 2 is a detailed sectional elevation of a porti not the apparatusjshown in Fig. 1 on a larger scale; M

3 is a cross-sectional viewshowing features which t be m iwt e ne m q im Q h iii ii it U ig. 4"is"across s e ctional view taken along the putt- 14 of Fig. 1';

es artin t 'the Pr se t invention, t tralization'of organic sulphonic acids for the productien eI' suriace-active agents is carried out by 28 PP? ESQ i 'mecntmtallv cir ed and agitated mass or" reaction prodta at? s i as e pi' ti e to ma n Water wer 9l.@ l.99 ?9?? w i h r to b nde state e -hrateew tt n e term asj sed here n) in liquid phase until the reaction s s m'als e whe t ppn th s is i ha d nt? 9 1? of 10W?! ,p fi l t Flash (11f a c ntroiied M punt of water. in this way the temns eter 9 lfi fi i owe by direQt at exchange, i. e., the heat required 101 vaporizaco nppsition of the final product is readily cont rglled and adjusted, and objectionable Ioaming cf the fluid mass-which premature volatllizatign of water might cause is prevented. By

proper regulation of the ratio of the recycle rate to the input rate, objectionable aeration of the mass and foaming may be prevented even when neutralizing agents are used which produce CO2. A high recycle rate is made economically feasible in the present invention by passing the returning stream in indirect heat transfer relation to, and preferably surrounded by, the stream withdrawn from a body of reaction product maintained in the flash vessel.

The term organic sulphonic acids is meant to include those substances in which the SO3I-I or OSO3H group is attached to an organic radical and which, when neutralized, have surfaceactive properties and may be used as detergents, wetting, emulsifying, dispersing, penetrating agents, etc., such as, for example, sulfates and sulphonates of long chain aliphatic hydrocarbons, higher fatty alcohols, long chain fatty acids, polyhydric alcohol, esters of fatty acids, alkyl ethers of polyhydroxy compounds, mixed aromatic and aliphatic hydrocarbons and the like.

The term neutralizing agent includes those substances capable of neutralizing organic sulphonic acids and may be taken from the group consisting of alkali metal and alkaline earth metal hydroxides and salts of these metals with weak acids such as carbonates and bicarbonates, aqueous ammonia, and organic bases such as the alkanolamines. It is generally preferred to employ caustic soda or soda ash as the neutralizing agent in the present invention where sodium salts are being manufactured.

The apparatus of the invention in which the process is preferably carried out comprises essentially an evaporator or flash cooling vessel having a vapor line communicating with the upper part thereof and a liquid circulating system having an inlet communicating with the lower part of the vessel and an outlet in the free space within the vessel a substantial distance above the inlet. A power driven impeller is provided for flowing a liquid stream of reaction product through the circulating system at a high rate and also for agitating it so that the flow is very turbulent. Pipes are provided for feeding the acid and the neutralizing agent into the circulating turbulent stream where thorough mixing is assured. The outlet of the circulating system is provided with means for varying the size of the discharge orifice whereby the pressure on the circulating mass between the impeller and the orifice can be controlled. A product discharge line is provided which may communicate either with the lower part of the vessel or the suction side of the circulating system. Preferably an automatic liquid level control is used to maintain a constant head of liquid in the vessel.

Referring now to Fig. 1 of the accompanying drawings, reference numeral l represents a cylindrical evaporator or flash cooling vessel adapted to maintain a fluid body of reaction products in the lower portion thereof. Vessel i has a flanged central outlet 2 providing passage through bottom wall 3. Secured to outlet 2 is an outer flanged draft tube 4 of such length that the annular space 3a between the outer draft tube 4 and an inner draft tube 5 creates sufficient pressure due to hydrostatic head at the lower end to keep water in liquid phase. In other words, there is a net positive suction head above vapor pressure. Secured to the lower flange of draft tube 4 is a casing 6 having a toroidal cavity 1 of substantially U-shaped vertical section. The inner draft tube 5 extends into cavity 1 but terand thus servin to reduce minates short of the bight thereof so that material fiowing downwardly through the annular space 3a, upon reaching the casin 6, is directed upwardly through the inner draft tube 5 which is substantially longer than outer draft tube 4 and extends into the free space of vessel l.

The requisite force for causing motion of the stream of liquid material upwardly through the inner draft tube is provided by the motion of an impeller 8 which is keyed to the shaft of a driving motor 9. Reagents are introduced into and dispersed inthe moving stream in the region of the casing 6, and in the violent turbulent stream which rises away from the impeller in the inner draft tube, they are thoroughly contacted. The reaction takes place sufiiciently rapidly under these conditions that it is practically completed within the inner draft tube. Since the neutralization takes place between reagents dispersed in a mass of cooled reaction product, the heat of reaction is also dispersed throughout the'mass, thereby preventing localized overheating and uncontrolled pH with all their attendant disadvantages.

In the upper outlet ill of the inner draft tube 5 is a conical head I2 which is adjustable in elevation with, respect to rim Iii by means of an external wheel 13, thus providing an orifice of adjustable area. By adjusting the area of the orifice the pressure on the mass in the inner draft tube 5 can be regulated and controlled as required to prevent premature vaporization or swelling within tube 5 and also to produce the required spray action to afford surface for vaporization and/ or degasification when the liquid issues into the free space in the vessel.

The stream of hot reacted material is discharged above the liquid level in the vessel l into a zone or region of pressure substantially reduced from that inside the draft tube Upon being subjected to the reduced pressure, a controlled amount of the water carrying the reaction products is flash evaporated, absorbing the heat required for vaporization from the mass its temperature by any desired amount.

The vessel 1 may be provided with suitable means to prevent entrainment of liquid in the vapor leaving the vessel, e. g., bafiie plates or the like.

A vapor line l4 connected at the upper wall [5 of the cylindrical vessel communicates with a condensing system (not shown) which serves to maintain the absolute pressure on the system at a desired level. Finished products are removed from the system by pipe 15 which is shown near the bottom of the cylindrical wall of the vessel 1, but it is apparent that it could be located anywhere below the liquid level in vessel I or in the wall of the draft tube 4 any place above the level of introduction of either reactant.

The condensing apparatus used to maintain the absolute pressure, usually a vacuum, may be chosen from a large class, for example any of the types commonly used in evaporation and dis-- tillation arts and in the reduction of back pres-- evolved in the reaction, for example, carbon dioxide.

Referring now to Fig. 2 of the drawings, inner draft tube 5 is secured to and spaced from the bottom of outer draft tube 4 by vanes [1. The lower end 5a of draft 'tube 5 is preferably made separate from the tube proper and permanently mounted in casing 6 by vanes 18 which extend upwardly in the center cavity almost to the impeller 8. Above the impeller are additional vanes 19 in the inner draft tube 5.

A supply line 20 is provided for introducing one of the reagents into the downflowing material in the annular space 3a. The downward flow is reversed in the toroidal cavity 1 and rotation of the fluid mass is inhibited by vanes l1, l8, and [9. This arrangement assures turbulent flow and violent agitation in the region of the impeller where "the other reagent is injected through nozzles 22, (see also Fig. 5). These nozzles are showndischarging into the inner draft tube at the blade tips of the impeller 8 but they may discharge either up or down stream from the impeller provided the mass is suficiently turbulent to effect rapid dispersal of the other reagent through the cross section of the liquid stream whereby the temperature of the mass is maintained substantially uniform notwithstanding the evolution of heat which results from the reaction.

The pressure in the inner draft tube is controllable by elevating and lowering the movable head I2. With introduction of one of the reagents upstream from and the other at or near the impeller such adjustability of process conditions insures that suflicient pressure may be maintained in the inner tube to prevent flashing prior to discharge of the volatile materials therefrom, and permits completion of the reaction under the desired condition of turbulence, temperature, pH and homogeneity.

A significant feature of the apparatus is that it makes economical and practicable a high ratio of recycle rate to input rate. 'One advantage of a high ratio is that an exothermic reaction can be carried out with a minimum temperature change and at the optimum temperature. In neutralizing the monosul-phate of coconut oil fatty acid monoglyce-rides with aqueous sodium hydroxide, for example, it is desirable that the temperature of the neutralized product not substantially exceed about 110 F. By maintaining a ratio of about 60/1 it is possible "to limit *thetemperature differential, as measured by thermometers in the space 311 and tube 5, respectively, to less than 2 F. Another advantage is that the relative volume of gas liberated in the reaction can be kept sufficiently low that the product does not foam or swell objectionably and the pumping action of the impeller is not interfered with. A further advantage is that better mixing is obtained with greater homogeneity in the reaction product.

Referring now to Fig. 3 of the drawings, a supply line 24 is shown which discharges into the outer draft tube, 1. e., into annular space 3a, and may be used for the introduction of desired builders, addition compounds and the like into the moving stream of reaction products. A nozzle 26 having its discharge end opening into the inner draft tube 5 may be utilized for collecting samples of the reacted material for analysis to determine the need for adjustment of the rate of introduction of any of the reagents, addition products, or the like, so as to yield a finished product of desired composition. Tubes 28 and 30 which have their discharge ends opening into the inner draft tube and the annular space, respectively, may be utilized to carry equipment such as thermometers or Bourdon tubes or diaphragm gages and the like for the measurement of tem- 6 peratures and pressures in the circulating liquid stream of material.

Fig. 4 depicts vanes 32 which serve to maintain the position of the inner draft tube 5 within the upper end of draft tube 4.

While the points of introduction of the reagents into the system are not critical in the strictest sense, it is generally desirable to introduce at least one of the reagents at or down stream from the impeller, so that the principal reaction may take place in the region of highest turbulence and maximum pressure, where foaming and flashing are kept at a minimum and the reaction mass is maintained substantially homogeneous until the reaction is considerably advanced or completed. The streams of both the reagents may be introduced at or near the impeller or one may be introduced near or at the impeller and one upstream. Which of these methods is preferred can be dictated best by the properties of the materials involved. For example, where the acid mix to be neutralized in continuous reaction contains a substantial amount of free sulphuric acid, it is oftentimes desirable that it be added to the stream at some distance from the impeller, to prevent the wellknown deterioration which results when acids, particularly strong acids, are placed in concentrated quantities in contact with metal parts. In such cases it may be most desirable to introduce the acid upstream from the impeller so that it becomes dispersed in the downflowing stream of reaction products before reaching the impeller where the alkali may be introduced. Thus the entire region of the turbulence is utilized to the best advantage in mixing the reagents and the only material which may exist in local excesseven briefly, at the impeller blade is the relatively non-corrosive alkali.

Another considerationof valueto the operation exists in that some reagents are more injurious to the reaction products than others, and in view of this it may be desirable that the least harmful of these be added upstream and be permitted to mix with the circulating stream of reaction products. In the neutralization of organic sulphonic acid with aqueous caustic sodaor soda ash for example, the rate of hydrolysis of certain types of organic residues in the neutralization product is considerably more rapid .in the presence of alkali than in the presence of acid; hence it is advantageous to introduce the acid up stream and the alkali at the impeller.

While the contactor described is of the type which comprises an internal impeller for causing motion of the circulating fluid, it should be understood that apparatus similar in effect but different in design may be employed to accomplish the same result. Thus, devices embodying the principle utilized in centrifugal pumps, as well as mechanisms of the positive-displacement variety, may be employed in place of the apparatus utilized in the lower portion of the casing 6 in Fig. 1. In any case, however, the heat transfer relation, and preferably the concentric arrangement, of the feed pipe to and the discharge pipe from the pump is an essential feature of my apparatus. With this arrangement a minimum hydrostatic head above the pumping device is required to suppress vaporization or flashing in the pump suction, i. e., the required net positive suction head above the vapor pressure of the volatile component is kept at a minimum.

The following example of typical operation in 7 V accordance with the invention is included to illustrate but not to limit the invention: 7

1146 parts (by weight) per hour of a mixture containing approximately'50% sulfuric acid and 50% sulfated monoglyceride ester of coconut oil fatty acids are continuously introduced at 120 F. through pipe 20 of an integral contactor-flash cooler of the type shown in the drawings. 3,023 parts per hour of a caustic soda solution of approximately 21% strength are added at 100 F. through nozzles 22 and the resulting mixture of reagents and circulating reaction products subjected to the violent flow conditions in the inner draft tube resulting from the action of the impeller. 625 parts per hour of a solution containing approximately 20% tetrasodium pyrophosphate and approximately sulfuric acid are added in the inner draft tube via nozzle 26, and become admixed thoroughly with the reacting mass. The reaction products are sprayed through orifice l0 into the vessel i where a vacuum is maintained of from 26 to 28.5 inches of mercury. 886 parts per hour of flash steam are removed to the condenser via vapor line [4, and 3,908 parts per hour of the solution in the vessel are removed by pipe It. The rate of flow through the inner draft tube is approximately 468,000 parts per hour, and the highest temperature increase in the circulating stream resulting from the heat of reaction is less than 2 F.

The term liquid as used herein is intended to include within its scope true solutions, colloidal solutions and suspensions of solids in a liquid vehicle. 7

Present application is a division of copending application Serial No. 31,861 filed June 9, 1948.

What is claimed is;

1. An apparatus comprising a flash cooling vessel providing an enlarged chamber having two vertically elongated concentric tubes opening into the lower portion thereof, the outer tube opening into said chamber adjacent to the bottom wall thereof and being closed at its lower end, the upper end of the inner tube extending a substantial distance upwardly into said enlarged chamher and the lower open end thereof terminating short of the closed lower end of the outer tube to provide a passage from one tube to the other, a

power driven impeller mounted in the lower end of said inner tube, an adjustable valv adjacent to the said upper end of said inner tube in said enlarged chamber for varying the size of the orifice between the upper end of said inner tube and said valve through which the inner tube communicates with said enlarged chamber, pipes for feeding reactants to said tubes, and a vapor line communicating with the upper part of said enlarged chamber.

2. An apparatus comprising a flash cooling vessel providing an enlarged chamber having two vertically elongated concentric tubes opening into the lower portion thereof, the outer tube opening into said chamber adjacent to the bottom Wall thereof and being closed at its lower end, the upper end of the inner tube extending a substantial distance upwardly into said enlarged chamber and the'lower open end thereof terminating short of the closed lower end of the outer tube to provide a passage from one tube to the other, a power driven impeller mounted in the lower end of said inner tube, an adjustable valve adjacent to the said upper end of said inner tube in said enlarged chamber for varying the size of th orifice between the upper end of said inner tube and said valve through which the inner tube communicates with said enlarged chamber, pipes for feeding reactants to said tubes, a product line communicating with the lower part of said vessel for withdrawing liquid from the apparatus, and a vapor line communicating with the upper part of said enlarged chamber.

LOWELL A. LEDGETT.

References Cited in the file of this patent UNITED STATES PATENTS Number Name Date 1,000,689 Paterson Aug. 15, 1911 1,735,980 Sadler Nov. 19, 1929 2,474,592 Palmer June 28, 1949 FOREIGN PATENTS Number Country Date 592,289 Germany Feb. 5, 1934 OTHER REFERENCES The Refiner, vol. 21, No. 6, June 1942, page 37. 

1. AN APPARATUS COMPRISING A FLASH COOLING VESSEL PROVIDING AN ENLARGED CHAMBER HAVING TWO VERTICALLY ELONGATED CONCENTRIC TUBES OPENING INTO THE LOWER PORTION THEREOF, THE OUTER TUBE OPENING INTO SAID CHAMBER ADJACENT TO THE BOTTOM WALL THEREOF AND BEING CLOSED AT ITS LOWER END, THE UPPER END OF THE INNER TUBE EXTENDING A SUBSTANTIAL DISTANCE UPWARDLY INTO SAID ENLARGED CHAMBER AND THE LOWER OPEN END THEREOF TERMINATING SHORT OF THE CLOSED LOWER END OF THE OUTER TUBE TO PROVIDE A PASSAGE FROM ONE TUBE TO THE OTHER, A POWER DRIVEN IMPELLER MOUNTED IN THE LOWER END OF SAID INNER TUBE, AN ADJUSTABLE VALVE ADJACENT TO THE SAID UPPER END OF SAID INNER TUBE IN SAID ENLARGED CHAMBER FOR VARYING THE SIZE OF THE ORIFICE BETWEEN THE UPPER END OF SAID INNER TUBE AND SAID VALVE THROUGH WHICH THE INNER TUBE COMMUNICATES WITH SAID ENLARGED CHAMBER, PIPES FOR FEEDING REACTANTS TO SAID TUBES, AND A VAPOR LINE COMMUNICATING WITH THE UPPER PART OF SAID ENLARGED CHAMBER. 